Synthesizer for acetoxyacetyl chloride

Abstract

The utility model provides an acetoxyacetyl chloride synthesizer which comprises a first synthesis kettle and a second synthesis kettle, the top of the first synthesis kettle and the top of the second synthesis kettle are both communicated with a first metering tank and a second metering tank through pipelines, and the first metering tank and the second metering tank are both provided with feeding pumps. The bottom of the first synthesis kettle and the bottom of the second synthesis kettle are communicated with a rectifying kettle through pipelines, a rectifying assembly is arranged at the top of the rectifying kettle, and a discharge port is formed in the bottom of the rectifying kettle; the whole device is simple in structure, the two synthesis kettles can be alternately used, so that the production efficiency is effectively improved, acidic mixed waste gases such as sulfur dioxide and hydrogen chloride are not generated, the utilization rate of raw materials theoretically reaches 100%, the device completely conforms to an environment-friendly and pollution-free green process, the reaction process is mild, and the production cost is low. The reaction speed can be controlled by controlling the temperature and the catalyst input amount, the production operation is safe, the production cost is low, and the benefit is high.

Description

TECHNICAL FIELD

[0001] The utility model relates to the field of pharmaceutical intermediates and fine chemical industry, in particular to a synthesis device of acetoxy acetyl chloride. BACKGROUND

[0002] Acetoxy acetyl chloride is an important organic synthesis and pharmaceutical, pesticide intermediate.

[0003] In the pharmaceutical industry, acetoxy acetyl chloride is used for producing ioversol medicine, paclitaxel, roxatidine acetate

[0004] At present, there are three methods for preparing acetoxy acetyl chloride in the industry: thionyl chloride system, phosgene system and triphosgene system.

[0005] 1) Thionyl chloride system: under the catalysis of zinc chloride, acetoxy acetic acid is used as raw material, and thionyl chloride is used as ring-opening reagent for ring-opening chlorination.

[0006] CH3COOCH2COOH+SOCl2——CH3COOCH2COl+SO2+HCl;

[0007] This process has simple process operation and easy-to-obtain raw materials, and is a suitable synthetic route for industrial production; the disadvantage is that sulfur dioxide, hydrogen chloride and other acidic mixed waste gas are produced, the treatment cost is high, and it does not meet the current requirements of green and environmentally friendly process.

[0008] 2) Phosgene system: phosgene is used instead of thionyl chloride, and acetoxy acetic acid is used as raw material for chlorination. The reaction process is as follows:

[0009] CH3COOCH2COOH+COCl2——CH3COOCH2COCl+CO2+HCl;

[0010] This process does not produce sulfur dioxide, and phosgene is cheaper than thionyl chloride, but phosgene itself is a highly toxic chemical, which is toxic and inconvenient to transport and store.

[0011] 3) Triphosgene system: triphosgene is used as chlorinating reagent, and the catalyst is used to catalyze the chlorination of acetoxy acetic acid. The reaction process is as follows:

[0012] CH3COOCH2COOH+CO(OCCl3)2——CH3COOCH2COCl+CO2+HCl;

[0013] Triphosgene is stable at room temperature and has low toxicity, but when reacting, the temperature is high, triphosgene decomposes quickly and is difficult to control, the reaction is easy to lose control, and the risk is large, and the catalyst is difficult to recover, which is not conducive to industrial production.

[0014] With the increasing market demand for acetoxyacetyl chloride, it is necessary to develop a synthesis device with high yield, which can meet the needs of industrial production, and low cost, and meet the requirements of green and environmental protection process. Utility model content

[0015] The utility model aims at providing a synthesis device of acetoxyacetyl chloride to solve the problems of the prior art.

[0016] To achieve the above object, the utility model provides the following scheme:

[0017] The utility model provides a synthesis device of acetoxyacetyl chloride, including first synthesis kettle and second synthesis kettle, the top of first synthesis kettle and the top of second synthesis kettle all are passed through pipeline with first metering groove and second metering groove communication, first metering groove and second metering groove all are equipped with feed pump, the bottom of first synthesis kettle and the bottom of second synthesis kettle all are passed through pipeline with rectifying kettle communication, the top of rectifying kettle is equipped with rectifying assembly, and the bottom of rectifying kettle is equipped with discharge gate.

[0018] Preferably, the first synthesis kettle and the second synthesis kettle are provided with stirring structure and heat preservation structure.

[0019] Preferably, the top of the first synthesis kettle and the top of the second synthesis kettle are provided with a tail gas treatment assembly.

[0020] Preferably, the tail gas treatment assembly includes a graphene condenser, the graphene condenser is connected with a first separator, and the first separator is connected with a tail gas discharge pipe.

[0021] Preferably, the rectifying assembly includes a condenser, the condenser is connected with a second separator, and the second separator is connected with the rectifying kettle, a vacuum buffer tank and a discharge pipeline respectively.

[0022] Preferably, a reflux flow machine is arranged between the second separator and the rectifying kettle.

[0023] Preferably, a discharge flow machine is arranged on the discharge pipeline.

[0024] The utility model has the following beneficial technical effects compared with the prior art:

[0025] The utility model provides a kind of acetyloxy acetyl chloride's synthetic device, including first synthesis kettle and second synthesis kettle, the top of first synthesis kettle and the top of second synthesis kettle are all communicated with first metering tank and second metering tank by pipeline, first metering tank and second metering tank are equipped with feed pump, the bottom of first synthesis kettle and the bottom of second synthesis kettle are all communicated with rectifying kettle by pipeline, the top of rectifying kettle is equipped with rectification assembly, and the bottom of rectifying kettle is equipped with discharge gate;The whole device mechanism is simple, two synthesis kettles can be used alternately, to effectively improve production efficiency, without sulfur dioxide, hydrogen chloride and other acidic mixed waste gas generation, theoretically raw material utilization rate reaches 100%, completely meet the green process of environmental protection and pollution-free, reaction process is mild, can be controlled by temperature and catalyst input amount Control reaction speed, production operation is safer, production cost is low and benefit is high. BRIEF DESCRIPTION OF DRAWINGS

[0026] In order to more clearly illustrate the technical scheme in the embodiments of the present application or the prior art, the drawings needed in the embodiments will be briefly introduced as follows. Obviously, the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained without creative labor on the basis of these drawings.

[0027] Figure 1 The synthetic device structure diagram of acetyloxy acetyl chloride provided by the utility model. DETAILED DESCRIPTION

[0028] The technical scheme in the embodiments of the present application will be described clearly and completely in combination with the drawings in the embodiments of the present application. Obviously, the described embodiments are only some embodiments of the present application, not all embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0029] The utility model aims at providing a kind of acetyloxy acetyl chloride's synthetic device to solve the problems existing in prior art.

[0030] In order to make the above-mentioned purposes, features and advantages of the present application more apparent and easy to understand, the present application will be further described in detail in combination with the drawings and specific embodiments.

[0031] Embodiment 1:

[0032] The embodiment provides a kind of acetyloxy acetyl chloride's synthetic device, such as Figure 1As shown, it comprises a first synthesis kettle 1 and a second synthesis kettle 2, the top of the first synthesis kettle 1 and the top of the second synthesis kettle 2 are communicated with a first metering tank 3 and a second metering tank 4 through pipelines, the first metering tank 3 and the second metering tank 4 are respectively provided with a feeding pump, the bottom of the first synthesis kettle 1 and the bottom of the second synthesis kettle 2 are communicated with a rectification kettle 5 through pipelines, the top of the rectification kettle 5 is provided with a rectification assembly 6, and the bottom of the rectification kettle 5 is provided with a discharge port 51.

[0033] As an embodiment, the first synthesis kettle 1 and the second synthesis kettle 2 are respectively provided with a stirring structure and a heat preservation structure, so as to realize the effects of stirring and mixing and heat preservation.

[0034] As an embodiment, the top of the first synthesis kettle 1 and the top of the second synthesis kettle 2 are respectively provided with a tail gas treatment assembly 7.

[0035] As an embodiment, the tail gas treatment assembly 7 comprises a graphene condenser 71, the graphene condenser 71 is connected with a first separator 72, and the first separator 72 is connected with a tail gas discharge pipe 73, so as to treat the tail gas.

[0036] As an embodiment, the rectification assembly 6 comprises a condenser 61, the condenser 61 is connected with a second separator 62, and the second separator 62 is connected with the rectification kettle 5, a vacuum buffer tank 63 and a discharge pipeline 64 respectively.

[0037] As an embodiment, a reflux flow machine 65 is arranged between the second separator 62 and the rectification kettle 5, for the reflux after separation.

[0038] As an embodiment, a discharge flow machine 66 is arranged on the discharge pipeline 64, for product discharge.

[0039] The utility model provides a kind of synthesis device of acetyloxy acetyl chloride, and its working principle is as follows: 1000kg of 70% glycolic acid is pumped into first synthesis kettle 1 or second synthesis kettle 2 by feed pump, acetyl chloride is pumped into first metering tank 3 by feed pump, and chlorobenzene is pumped into second metering tank communication 4 by feed pump, the raw materials in first synthesis kettle 1 are stirred by starting stirring structure, the stirring speed is 65-75 revolutions / min, acetyl chloride is added dropwise at 0-45 DEG C, after dropwise addition is completed, heat preservation reaction is carried out for one hour, then catalyst is added, and the temperature is increased to 60-70 DEG C, chlorobenzene 5000kg is added dropwise, after dropwise addition is completed, heat preservation reaction is completely, first synthesis kettle 1 and second synthesis kettle 2 can be used alternately in this process, tail gas is treated by tail gas treatment component 7, and the tail gas is mainly hydrogen chloride, hydrochloric acid is prepared by three-stage absorption treatment, after synthesis is finished, vacuum transfer is carried out to rectifying kettle 5, rectification is carried out under vacuum-0.095MPa, temperature 120-130 DEG C, a small amount of front distillation acetyl chloride is first distilled, product acetyloxy acetyl chloride is then distilled, and then middle fraction is discharged, the bottom material of rectifying kettle 5 is distilled to benzoyl chloride distillation kettle by vacuum transfer, and benzoyl chloride is distilled, distillation is carried out under vacuum-0.095MPa, distillation temperature is 130-150 DEG C, and product and byproduct are packaged after chromatographic analysis is qualified.

[0040] The utility model has been described with specific examples, and the above examples are only used to help understand the method and core idea of the utility model; meanwhile, for those skilled in the art, according to the idea of the utility model, there will be changes in specific implementation mode and application range. In conclusion, the content of the specification should not be understood as a limitation of the utility model.

Claims

1. An apparatus for the synthesis of acetoxyacetyl chloride, characterized by: The device comprises a first synthesis kettle and a second synthesis kettle, the top of the first synthesis kettle and the top of the second synthesis kettle are communicated with a first metering tank and a second metering tank through pipelines, the first metering tank and the second metering tank are provided with a feeding pump, the bottom of the first synthesis kettle and the bottom of the second synthesis kettle are communicated with a rectifying kettle through pipelines, the top of the rectifying kettle is provided with a rectifying assembly, and the bottom of the rectifying kettle is provided with a discharge port.

2. The apparatus for synthesis of acetoxyacetyl chloride according to claim 1, characterized in that: The first synthesis kettle and the second synthesis kettle are provided with stirring structures and heat preservation structures.

3. The apparatus for synthesis of acetoxyacetyl chloride according to claim 1, characterized in that: The top of the first synthesis kettle and the top of the second synthesis kettle are provided with a tail gas treatment assembly.

4. The apparatus for synthesis of acetoxyacetyl chloride according to claim 3, characterized in that: The tail gas treatment assembly comprises a graphene condenser, the graphene condenser is connected with a first separator, and the first separator is connected with a tail gas discharge pipe.

5. The apparatus of claim 1, wherein: The rectifying assembly comprises a condenser, the condenser is connected with a second separator, and the second separator is connected with the rectifying kettle, a vacuum buffer tank and a discharge pipeline respectively.

6. The apparatus of claim 5, wherein: A reflux flow machine is arranged between the second separator and the rectifying kettle.

7. The apparatus of claim 5, wherein: A discharge flow machine is arranged on the discharge pipeline.

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